Glycobiology is now being widely viewed as an important and frontier branch of biochemistry and medicine. New and exciting roles for glycoproteins and proteoglycans in biochemistry are being discovered at a great rate, but the field has been handicapped by the lack of methodologies that can provide measurements at high sensitivity. This proposal deals with a concerted effort to change this general deficiency and provide considerably more sensitive techniques in the area. The cornerstones of the proposed approach are unique fluorogenic reagents that will enable reliable tagging of various glycoconjugate fragments (oligosaccharides and glycosaminoglycans) for a subsequent separation by high-performance capillary electrophoresis and detection/measurement using laser-induced fluorescence. This proposition is further reinforce by incorporating such sensitive techniques into the overall analytical schemes featuring an effective handling of the nonogram quantities of analyzed glycoconjugates, followed by microscale enzymatic treatment, chromatographic separations, and, finally, the above-mentioned high- efficiency electrophoresis and laser-assisted detection. Consequently, the proposed research will enable the biomedical investigators to perfor the measurements on glycoconjugates which are several orders of magnitud more sensitive than the methods available today. Whereas, the initial experiments will mostly involve model glycoconjugates, the later stages of this proposed research will be oriented toward certain challenging problems of contemporary biochemistry: receptor proteins and other important glycoconjugates from the field of membrane biochemistry. The methodologies at the nanogram amounts of the initial glycoconjugate samples will yield capabilities of glycoform profiling, oligosaccharide mapping, leading further to sequence determinations. It is quite likely that the developed methodologies will also find some utility in biotechnological analysis where recombinant glycoconjugates are being increasingly explored.